Process of distilling glycerin.



esses' followed heretofore it has been c .10

, against'the bodies of' glycerin containedinthe stills. lConsequently while the desired plates Vacuum, or evenga perfect vacuun'iJ mightbe p lied throughl pipes j UNiTED STATES 'PATENT einen.

FRANK J. woon, oF--N'EW YORK, N. Y., A'ssIGNoR 'ro- MARX AND ia'AwoLLE, 0F NEW YORK N Y.\, A/CORBORATION 0F NEW YORK. p

PRocEss on Drs'rILLING GLYGEBIN'.

No. santas. specification of Letters Patent. Patented March 1o, 190e.

Application mea nach 22,1905. sei-iai No. 251,520.- v

To all 'whom 'it may concern: l which the ressure would Vbe relieved would Be it known that I, FRANK 1J. Woon, a citi not be suiiileient to avoid decomposition. zen ofthe United States, residing in the city he essence of my invention is economyof New York, State of New York, have inof steam supply and consequent saving of. 1.* vented a certain new and useful yIm roved `fuel necessary to distil agiven quantit of ee Process of Distilling Glycerin, of which' the glycerin. n carryingcut the process am` ollowingisaspeciiication. ,j enabled to employ a plurality of .stills and In distilling glycerin according to the pro condensers connected 1n series and to which'. l

ngi-V a single column of steam`is supplied, b seV tomary to employ a single still, or a plurality mingling the steam with the several b dies e5 of stills each having a separate steam supply.. of glycerin that its passage into and through rSo far as I am `aware there has been no the stillsisaccelerated rather than retarded. process devel'ofped. which contemplated the 'The economy in steam, su ply is aided by employment o a plurality ofstills connected utilizing the' heat given 0H y the glycerin in in series and :successive y supplied with a its condensation to generate steam which 7,0 single lcolumn of steam to be mingled with may be vadded to that supplied to the stills. the glycerin-contained inthe several stills. i In the accompanying drawing I have The reason for this is that it has'been cusshow fappropriate mechanism for carrying tomary to introduceA or inject thefsu erout the process-,Figurelillustratingtheentire heated steam into theglycerin throug a system in conventional arrangement, `and pipe entering the still at the bottom thereof Fig. 2 a detail of one of the stills., or beneath the( surface ofthe body, of glyc Referring to the draw' E and E are erin. Consequently the line of lcom munivevaporators in"double effect arrangement. cation through a series of such stills would S, S, S- are' stills, -each comprising a al/so be through the, bodies of glycerinin the glycerin reservoir `F supplied at vX and 80 stills, and therefore a single column of steam on Which is mounted acylindrical casing H to be intimately mingled with Vthe glycerin in containing vertically disposed' tubes l), su all of the stills in lsuccession, `would have to ported. by.` plates a, a. The tubesof t e. be underrhigh lpressure in orderton overcome .first still communicate throu h an opening the hydrostatlc pressures of the bodies of in` the top of the casing W1th 'a pipe t 85 glycerin. Thiswould obviously cause the through which the steam is supplied from glycerin to be vaporized very slowlylunless it evaporator E. In the lower portions of wereheated to afdegree which might occasion the, tubes are spiral plates T while above the its decomposition. These'fa'ctsl alone vwould plates are the extremities of nozzles e extendprecludesup lying a single column of steam ing dojwnwardlyin the tubesbfrom a manifold to a series o 'stills vin which the steam and t', 'in communication'v with the res'ervior F,

glycerin were mingled inthe manner-stated. a centrifugal pump Isuppl ing glycerin ton yBut aside Afrom these points, 'although ofthe manifold and nozzles.' he normal level equal importance, is the fact thatv where a of the glycerinin tanks F isiwell below tl'ieglf. plurality of stills Vis emplo ed a uniformdevtops of the latter so that ample space 1s left 595 vgrec of vacuum .is essentia This should be for 4the passa e of thesteam and glycerin aboutf'28 or129 inches since that pressure vapors from. t etubesfb tothe pipes t lead- 'will permit of' eifectively'distilling gl cerin ing to 4the glycerin condenser-s C, C', 0.' Y hile, avoiding its', decomposition. k T` e ac- Throu hpipes f high pressure steam from tion of a vacuum pump lconn'ect'edto a series boiler enters the interior of tlie casings H 10Q of stills ofthe known construction would be and surrounds the tubes b.

.- The. lycerin fondensers C, C', C contain inclosing'a s ace for hot watersup- Tubes 7c are 'vercreated in the last still, .or that ad'acent the .tlcally mounted in the plates Z and .are thusf105 pump,there would be material vdi erencesin surrounded by the hotl wat-er andaiord' the degrees of vacuum in the receding #communication from'pipe t to the s ace in stills, varying according tothe -heig vts of the the condensers beneath the lower p ates Z g5 several bodies of glycerin, with the probable constituting distillate tanks -havingloutlets result that in .therststill the extent to X.l ,Pipes t connect the distillate tanksllo with Lthe succeeding `stills S S. From points above the water level e of the hot water spaces of these condensers pipes R is proper since at that temperature moreA as against are shown leading to the steam pipe t, a pressure regulator R being indicated near the intersection. TheY steam and glycerin condenser C is of substantially'the same construction as the glycerin condensers except that it is supplied with a circulation of cold water by pipes XW. A pipe 1 establishes communication Abetween this condenser and evaporator E, and a pipe V' connects it with the vacuum pump V.

Preparatory to beginning the process the tanks F of the stills are supplied to about two-thirds of their capacity with hot glycerin. The vacuum pump is put in operation to create vacuum of about 28 inches in the stills their tanks and tubes, and in the tubes of the condensers and in the evaporator E. be established throughout any number of stills and condensers since the line of communication from the evaporator E to the` pump isy not at any point obstructed by a body of glycerin. By adjustment of the pressure regulator R the vacuum in the hot water spaces of the condensers C, C', C, is reduced to about 16 inches so that the Water will boil at about175 degrees F. I have selected this degree of pressure yfor the reason thatif the pressure Ain the hot water space ofthe condensers C and in pipe R were to be the'same as that in the stills, 28 inches, the water would boil at avery low temperature or about 101 F. This would create a lower temperature in tubes k than is necessary for condensing the glycerin, and as the steam and vapors passed through the tubes the steam would be cooled to such an extent that a great quantity of heat would be ref. quired to superheat it before it wouldl bev available for ldistilling in' the succeedin still, since for that purpose its temperature s ould be between 310 and 350 degrees F. `the other hand, the pressure in the vapor spaces of the condensers was too -great the steam and lycerin` passing through the tubes would e at such a high temperature that all of thejglycerin might not be condensed'. Consequently I have determined thatl a temperature'of about 175 degrees F.

heat Will be maintained in the steam and yet the glycerin will be fully condensed.'`

To obtain `this temlperature a pressure of about 7 pounds abso ute or vacuum of about 16 Ainches inV pipe R is essential. I accordingly AWeight the pressure regulator R so that with'28 inches of vacuum, or about one pound absolute, in the stills, it willjbe seated ipe R. When the vacuum pump isstarted 1t exhausts the air from the stills', their tanks and tubes, `the tubes 7c of'th'e condensers and This uniform vacuum may readily' If, on

land enters apress'ure of 7 pounds or less inthe evaporator E', but the pressure in pipe R will not be affected by reason of the yweight which holds the regulator valve to its seat. But when the ressure .in the stills has been reduced to a out 6.7 pounds (the approximate difference in the pressures) the pressurein pipe R will unseat the valve and this pressure will be lessened until itis approximately 6.7 pounds higher than that of the stills. As the lessening of the pressure in the stills continues the pressure in pipe R also continues to' be lessened, but the differencey of approximately 6.7 pounds between "the two pressures remains constant. Consequently when .the desired` vacuum of 28 inches in the stills is obtained the vacuum in pipe R Willbe about 16 inches.

In commencing the process it will be assumed that the evaporator E contains I sweet water from a previous distillation supplied to it through pipe 1 from the steam condenser C". It is desirable that the im urities contained in this sweet Water shal not become mingled with the glycerin to be distilled but that only steam generated bfrom pure water be used. I therefore supply the evaporator E with pure water. Steam from the boiler B vaporizes the `sweet water in levaporator E and' this vapor passes to the steam space of evaporator E and vaporizcs vthe pure water therein, the pure steam generated by this double effect evaporating system being conducted through pi e to the irst of the stills and there minglDed with the glycerin.

It may here be noted .that Yalthough the steam supplied to the evaporator E from the boiler is at the same temperature, and is, in fact, the same steam, as that employed for distilling'the glycerin in the stills, yet the glycerin contained in the sweet water will not e distilled in the evaporator E for the reason that rit is combined with water which will evaporate first at temperatures from 110 to 160 degrees F., while the glycerin requires a vaporizin temperature of 280 degrees F. or more, an for the further reason thatthc4 evaporator E is being continually supplied withthe sweet water. When the evaporator E hasoperated sufficiently long the supply of sweet water and of steam may be cut off and the accumulated glycerin withdrawn.

The ure steam from the eva orator E passes t ough pipe t to the stil S and entering at the to -of the casing H passes down the tubes b. e pum P is started and the glycerin is thereby Wit drawn from tank F the manifold and nozzles i. 'Duringl its gravitation the glycerin is heated, and

y the steamjet is superhea'tedr by steam under about 150 pounds pressure passing from the boiler through pipe f into the space of the cylinder H around the tubes b, which are thus heated to about 370 de rees F. On passing out of the nozzlesgthe g ycerin unites .sanas-s With the steam and their combined vvapors under the action of the superheating steam they are subjected to a W feliects their. complete and residue dropping back into the tankF.

The temperature of the water contained in condenser C is about 175 degrees F. which, under the vacuum there maintained, is sufficiently cool to condense the glycerin vapors but sufficiently hot to maintain the steam vapors, as reviously explained. Consequently the istilled and condensed glycerin falls to the /receptacle at the bottom of the "condenser from which it may be withdrawn peat through, pipe X, while the steam passes throu h 1pipe t to the still S in which are `re- .y glycerin from the reservoir, its mingling with the. steam, and superheating ofthe steam.-

vWhile I specify superheating the'steam at each distillation, yet the essential oilice of t e hi h pressure steam supplied throu h pipes jg is the heating of the glycerin, as t e steam would be available for continued and successive use so long as it remained above the saturation point, and would) not itself require superheating before mingling with the glycerin ateach distillation. From the foregoing it will be seen that any number of`l 35 ,stills might be employed in each of which a body of glycerin could be distilled with only one column of steam for successively minglin with the glycerin in the several stills, as the steam would beof the same value in all of the stills. By my invention, however, I may do more than maintain the steam sup ply brou ht to the iirst still from the evaporator. may increase its volume by adding er spaces of the condensers C, C', C.'.

pplied through and consequently 1t will give up Whenit condenses. As it condenses passage throughthe s heat by its rounded by the Water at a temperatureto effect its condensation, this water will take I up the heat given oli" by the glycerin and will attain the boiling Which the regulator R y point, the steam generated plassin through pipe R to pipe t for use in t 'e stl within pi has attained a certain degree o pressure for may be adjusted,

temperature of the water in the condenser. Obviously the steam thus generated in the condenser may be cori/ducted elsewhere than to the steam-passing to the stills.

" The actions in the sillsS, S", and their re-A e described steps of withdrawing.`

In' vaporizing the glycerin absorbs: the heat of the `high pressure steam su tubes 7c, which are surs. Tlns auxiliary steam sup ly may l however, be confined e l? uhtil it series of successive distillations,

s peetive condensers are' the same as those statedv 'with 'reference to'still S and its con-- denser, each still containing glycerin which is vaporized and mingled with asingle'column1-, 'oi steam, the flow of the steam being A.inthe -same direction as the gravitating cellfimns ofl glycerin with which it unites, its value' being maintained throughout the system,`only Vits temperature varying since each glycerin condensation lowers itfrom the superheatedto near the saturation oint, and each condenser collecting distilled and condensed glyc erin While malntaining the steam and gen`- eratin additional steam by the condensation o the glycerin.

4F rom the last of the glycerin condensers C the steampasses to' the cold Water condenser C where the steam and the glycerin which may be entrained with it are condensed, after which the sweet Waterpasses to the evaporator E as before described.

i I am aware that there have been various means devised and practiced for separating or extracting glycerinfrom solids-.or liquids in which it is contained, such as fats, the residueA from soap.'V manufacture; vinass'es, etc., and that inasomeof the modesioi". treating these residues steam has been injected into or mingled with. the glycerin-containing materials other than against the 'resistance of ythe 95 hydrostatic pressure of 'the material, but these known methods merely separate glycerin which must be subsequently distilled to derive what is known as. chemically pure glycerin, and are therefore not germane to 100 the multiple effect of the steam supply, that is, the utilization -of a single jet of steam for successively combining with, and effecting the distillation of, the glycerin contained in a plurality of stills.

I claim as my inventionm l 1. The process of effecting a series of glycerin distillations, consisting of successively combining a plurality of bodies of glycerin with a sin le jet of steam of thestil s in which the bodies of glycerin are contained, and condensin the lycerin vapors obtained from each bo y of g ycerin.

2. In theprocess of distillin glycerin, successively combinin a single co umn of steam 115 with a plurality o bodies of gly-erin, and condensing the vaporizedv glycerin of each coinbination while maintaining the steam, the latter combining Witha succeeding body of glycerin. l 120 3. The process of distilling glycerin cony sisting of utilizing a single jet of steam for 'a combining with the steam`jet in each distillation a iloW-. ing vcolumn of glycerin, and condensing the 125 glycerin vapors of each distillation While maintaining the steam, the latter combining with a succeeding column of glycerin.

4. The rocess lof distillingi lycerin consisting 0f il) flowing through all eating columns ofl g ycerin in se- 13o f ries, successively' combining with the colerin, consisting of generating steam umns of glycerin a single jet of steam, and condensing .the vaporized glycerin of each column while maintaining the steam, the latter combining with a succeeding column of heated glycerin. l

5. The process of effecting a series of glycerin disti ations consisting of successivel combining flowing columns of glycerin wit a sin le jet of steam, superheating the com bine vapors at each distillation, and condensing the glycerin vapors obtained from each column of glycerin.

6. A step in the process of distilling) glycy the heat vgiven off bythe glycerin vapors in the condensation thereof.

7. In a glycerin distilling process, vaporizing the glycerin, condensing the va ors, generating steam by the heat given o by the glycerin in its condensation, and utilizing in the distillation system the steam thus genlerated.

i sisting of heating a flowing co umn of glycerin, combining steam with the glycerin, superheating the steam, condensing the glyc- -erin in ahot water condenser, and conducting the steam generated by the condensing glycerin to the steam prior to its union with the glycerin.

10. The process of distilling glycerin consisting of utilizing a single `jet of steam for a series of successive distillations, combining with the steam jet in each distillation a column of glycerin flowing in the same direction as the steam jet, superheating the steam at each distillation, condensing the glycerin vapors of each distillation,'and addinglte the steam prior to its union with the first column of glycerin steam generated by the glycerin in each condensation thereof.

11. The process of distilling glycerin consistng of utilizing a single jet .of steam for a series pf successive distillations combining with the steam jet-in each distillation a column of glycerin flowing in the same direction as the steam jet, superheating the steam at each distillation, condensing 1n a hot water condenser the vapor obtained from each column of glycerin, and conducting the steam generated by the condensing lycein to the steam prior to its union with t e first column of glycerin. l c

12.*In the process of distilling glycerin, the following steps: condensing the steam and .glycerin from a previous distillation, evaporating the sweet water thus obtained, and generating pure steam by the heat of the vapors ofthe sweet water.

13. In the process of distilling glycerin, the following steps: condensing the steam and glycerin from a previous distillation, evaporating the sweet water thus obtained, generating pure steam by the heat of the vapors of the sweet water, and conducting the pure steam to the still.

14. The process of distilling glycerin consistin of combining steam with glycerin and super eating the combination in the presence of a vacuum, and condensing the glycerin out of the steam byi causing its heat to be ab sorbed by a body of water which is in the presence of a vacuum less than that under which the lycerin is distilled, and utilizing in a succeeding distillation the steam maintained during they condensation of the glycerin.

15. The process of distilling glycerin consistin of combining steam with glycerin and super eating the combination in the presence of a vacuum of approximately 28 inches of mercury, condensin the glycerin by causing its heat to be absor ed by a body of water which is in the presence of a vacuum of approximately 16 inches of mercury whereby steam is generated from the condenser water, and utilizing the steam thus generated in the distillation ofthe glycerin. 4

, vFRANK J. WOOD.

- ANDREW C. JACKSON,

GEORGE MACINTOSH. 

